EP1378694B1 - Rupture disc assembly - Google Patents

Rupture disc assembly Download PDF

Info

Publication number
EP1378694B1
EP1378694B1 EP20030253952 EP03253952A EP1378694B1 EP 1378694 B1 EP1378694 B1 EP 1378694B1 EP 20030253952 EP20030253952 EP 20030253952 EP 03253952 A EP03253952 A EP 03253952A EP 1378694 B1 EP1378694 B1 EP 1378694B1
Authority
EP
European Patent Office
Prior art keywords
annular member
rupture disk
fluid
valve
annular
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP20030253952
Other languages
German (de)
French (fr)
Other versions
EP1378694A2 (en
EP1378694A3 (en
Inventor
Michael Stanley Decourcy
Connie Sue Williams
David Alec Williams
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Rohm and Haas Co
Original Assignee
Rohm and Haas Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Rohm and Haas Co filed Critical Rohm and Haas Co
Priority to EP05076038A priority Critical patent/EP1561521A3/en
Priority to EP05077882A priority patent/EP1640647A3/en
Publication of EP1378694A2 publication Critical patent/EP1378694A2/en
Publication of EP1378694A3 publication Critical patent/EP1378694A3/en
Application granted granted Critical
Publication of EP1378694B1 publication Critical patent/EP1378694B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K17/00Safety valves; Equalising valves, e.g. pressure relief valves
    • F16K17/02Safety valves; Equalising valves, e.g. pressure relief valves opening on surplus pressure on one side; closing on insufficient pressure on one side
    • F16K17/14Safety valves; Equalising valves, e.g. pressure relief valves opening on surplus pressure on one side; closing on insufficient pressure on one side with fracturing member
    • F16K17/16Safety valves; Equalising valves, e.g. pressure relief valves opening on surplus pressure on one side; closing on insufficient pressure on one side with fracturing member with fracturing diaphragm ; Rupture discs
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B17/00Methods preventing fouling
    • B08B17/02Preventing deposition of fouling or of dust
    • B08B17/06Preventing deposition of fouling or of dust by giving articles subject to fouling a special shape or arrangement
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B5/00Cleaning by methods involving the use of air flow or gas flow
    • B08B5/02Cleaning by the force of jets, e.g. blowing-out cavities
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K17/00Safety valves; Equalising valves, e.g. pressure relief valves
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16KVALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K27/00Construction of housing; Use of materials therefor
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00Fluid handling
    • Y10T137/1624Destructible or deformable element controlled
    • Y10T137/1632Destructible element
    • Y10T137/1692Rupture disc
    • Y10T137/1714Direct pressure causes disc to burst
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00Fluid handling
    • Y10T137/4238With cleaner, lubrication added to fluid or liquid sealing at valve interface
    • Y10T137/4245Cleaning or steam sterilizing
    • Y10T137/4259With separate material addition

Definitions

  • Unwanted materials may comprise byproducts, residues, polymers, scale, dusts, corrosion products, precipitates, or other solids, liquids or vapors. Unwanted materials may restrict process flows, initiate undesirable side reactions (such as stress corrosion cracking), seed polymer growth, and render secondary process devices - such as valves and instrumentation - inoperable.
  • the accumulation of unwanted material is costly in that it requires process downtime and manpower to remove these materials and to repair associated damage to the process equipment and piping that may have occurred.
  • hazardous situations can result when safety equipment, such as pressure relief devices, are isolated from the process through the accumulation of unwanted materials in the process connections to which they are attached.
  • a pressure relief device is disclosed in DE 31 02 828.
  • the device comprises a rupture disk retained between two annular rings.
  • the rupture disk extends across and seals a fluid conduit.
  • Condensation polymer forms when vapor-phase monomers condense onto equipment surfaces in the absence of suitable polymerization inhibitors and then undergo polymerization.
  • Monomers known to undergo condensation polymerization include but are not limited to (meth)acrylic acid and its esters, vinyl chloride, hydrogen cyanide, acrylonitrile, styrene, and other vinyl monomers.
  • One known method for combating condensation polymerization in the vapor spaces of process equipment is to maintain the surface temperature of the equipment above the dew point of the monomer(s); jacketing, insulation and electric or steam tracing of process equipment has been shown to be relatively effective in "open-flow" regions, i.e. regions where the vapor-phase monomer can freely flow away from the heated surfaces.
  • This approach is ineffective, however, in low flow regions such as process connections where the monomer vapors can stagnate and become trapped; this situation is further exacerbated when the process connection is a vessel nozzle, oriented vertically on the top head of the process equipment in question.
  • vapor-phase inhibitors have also been tried as a means for preventing condensation polymerization inside process equipment such as distillation columns.
  • examples of such inhibitors include SO 2 in hydrogen cyanide service and NPH in (meth)acrylic acid service. Because low flow regions, such as nozzles, are essentially stagnant, however, vapor-phase inhibitors tend not to flow into them and unwanted material accumulation can proceed essentially unabated.
  • FIG. 10 of the present application illustrates such an embodiment wherein a spraying and supplying means is employed in combination with a top head connection to which a relief device (typically a rupture disk and relief valve assembly) is attached. The insertion of a single spray nozzle into the process connection from below is illustrated; in this configuration, a liquid spray would be direct upward into the stagnant process connection.
  • a relief device typically a rupture disk and relief valve assembly
  • the installation of the spray nozzle is mechanically complex as well as invasive to the vessel, requiring a separate vessel penetration (not shown) and the positioning of the line(s) inside the vessel for supplying the liquid to the spray nozzle.
  • the elevation and alignment of the spray nozzle itself, as well as the flow rate and spray pattern are critical and, in practice, it is quite difficult to obtain the proper combination of these variables such that polymer accumulation is wholly prevented. While the effectiveness of such an arrangement could be improved through the use of multiple spray nozzle and an overwhelmingly large quantity of liquid spray, such an approach is costly and impractical in commercial operations.
  • the physical presence of the spray nozzle(s) and its supply line(s) create an undesirable obstruction in the process connection, thereby interfering with the free flow of material through the attached relief device, and these components themselves also create new surfaces for the accumulation of condensation polymer!
  • the direct impingement of pressurized spray liquid on the relief device may also cause mechanical fatigue, thereby shortening the service life of the rupture disk. Because of these limitations, the proposed process for inhibiting polymerization is impractical when applied to the small, low flow regions associated with process connections, such as relief lines.
  • a rupture disk assembly comprising a rupture disk and a rupture disk holder operatively engaging the rupture disk; wherein the rupture disk holder comprises a first annular member disposed in a downstream position relative to the rupture disk and a second annular member disposed in an upstream position relative to the rupture disk; wherein an outer peripheral portion of the rupture disk is sandwiched between the first annular member and the second annular member; wherein the second annular member includes at least one fluid port aimed at the rupture disk.
  • a rupture disk assembly comprising a rupture disk and a rupture disk holder operatively engaging the rupture disk; wherein the rupture disk holder comprises a first annular member disposed in a downstream position relative to the rupture disk, a second annular member disposed in an upstream position relative to said rupture disk and a third annular member disposed in an upstream position relative to the rupture disk; wherein an outer peripheral portion of the rupture disk is sandwiched between the first annular member and the third annular member; wherein the third annular member is sandwiched between the outer peripheral portion of the rupture disk and the second annular member; wherein the second annular member includes at least one fluid port aimed at the rupture disk.
  • process equipment is meant vessels, such as distillation columns, tanks and reactors, and process piping systems.
  • process connections is meant any extension of process equipment which can be utilized for the attachment of secondary process devices such as valves, instrumentation, pumps or pressure relief devices.
  • Process connections include, but are not limited to, studding outlets, piping branches (e.g., piping tees), manways, handholes and flanged nozzles.
  • a key component of the present invention is a flush ring, i.e. an annular member having one or more fluid ports, the one or more fluid ports serving to direct a flushing fluid inwardly of said annular device, preferably toward the axis of the annulus.
  • the annular member also includes an internal channel fluidically connecting the one or more ports to an external source of the flushing fluid. It is preferred that the annular member be of a constant external diameter. It is also preferred that the annular member be of a constant internal diameter. It is further preferred that the annular member comprises smooth and substantially parallel upper and lower surfaces of such a quality as to facilitate sealing when installed with conventional gaskets in a piece of process equipment.
  • flushing fluid Any gaseous or liquid material, compatible with the operation of the process, may be employed as the flushing fluid.
  • the flushing fluid may be supplied continuously or intermittently, as required.
  • the flush ring When installed in a low flow region, the flush ring serves to flush unwanted materials from the low flow region, thereby preventing their accumulation and avoiding the previously described processing difficulties associated with the accumulation of unwanted materials.
  • the flush ring may be optionally installed with a flow measurement / control device (such as a control valve, a needle valve or a rotometer) on the flush fluid supply connection. This serves to ensure proper flushing fluid flow is maintained at all times, as intended.
  • a flow measurement / control device such as a control valve, a needle valve or a rotometer
  • FIG. 1 illustrates one embodiment of a flush ring in accord with the present invention.
  • an annular channel and fluid ports consistent with the present invention are incorporated directly into a rupture disk holder.
  • a fluid flush may be provided to prevent the accumulation of unwanted material, such as condensation polymer, in the low flow region upstream of a rupture disk.
  • the rupture disk assembly 101 is representative of conventional assemblies used in industrial chemical processes and comprises a rupture disk 103 contained in a two-piece rupture disk holder comprising a first annular member 105 disposed in a downstream position relative to the rupture disk 103 and a second annular member 107 disposed in an upstream position relative to the rupture disk 103.
  • An outer peripheral portion 109 of the rupture disk 103 is sandwiched between the first annular member 105 and the second annular member 107.
  • the second annular member 107 includes a plurality of fluid ports 111 in its interior face 113 through which a flushing fluid may be passed.
  • the ports 111 are oriented at two different angles with respect to the axis 115 of the second annular member 107 in order to direct the flushing fluid (illustrated by the arrows) toward multiple points along the lower surface 117 of the rupture disk 103.
  • the flushing fluid is supplied via a connection 119 to a source of flushing fluid (not shown) and an annular internal channel 121 which is operably connected to each of the ports 111 by respective feed channels 123.
  • FIG 2 illustrates an embodiment of the flush ring in accord with the present invention wherein only two fluid ports are utilized.
  • fluid port 211a is oriented at a first angle with respect to the axis 215 of the second annular member 207 and conducts flushing fluid (illustrated by the arrow) toward a first area on the lower surface 217 of the rupture disk 203.
  • Fluid port 211a is supplied via a radially-oriented hole 225a and feed channel 223a in the second annular member 207.
  • the radially-oriented hole 225a serves to conduct flushing fluid from the connector 219a which is in turn connected to a source of flushing fluid (not shown).
  • fluid port 211b (located on the diametrically opposite side of the second annular member) is oriented at a second angle (different from the first angle) with respect to the axis 215 and flushing fluid toward a second area on the lower surface 217 of the rupture disk 203.
  • Fluid port 211b is supplied via a radially-oriented hole 225b and feed channel 223b in the second annular member 207.
  • the radially-oriented hole 225b serves to conduct flushing fluid from the connector 219b which is in turn connected to a source of flushing fluid (not shown).
  • Connector 219a and connector 219b may draw flushing fluid from the same source or may optionally use different flushing fluids - for example, one fluid may comprise water and the other fluid may comprise an organic solvent such as hexane, or alternatively, one fluid may comprise phenolic inhibitor solution and the other may comprise an oxygen-containing gas.
  • one fluid may comprise water and the other fluid may comprise an organic solvent such as hexane, or alternatively, one fluid may comprise phenolic inhibitor solution and the other may comprise an oxygen-containing gas.
  • Figure 3 illustrates another embodiment of the flush ring in accord with the present invention which, while functionally similar to the apparatus of Figs. 1 and 2, is an independent part.
  • This independent flush ring is used to prevent the accumulation of unwanted material, such as condensation polymer, in the low flow region, generally indicated as 327, upstream of a relief device assembly, generally indicated as 329.
  • the relief device assembly 329 is representative of conventional assemblies used in industrial chemical processes, one example of which is described in U.S. Patent No. 6,311,715.
  • the relief device assembly in this preferred embodiment comprises a reverse-buckling rupture disk 304 (contained in a two-piece rupture disk holder comprising a first annular member 305 and a second annular member 307).
  • Suitable reverse-buckling rupture disks are commercially available from Continental Disc CorporationTM, FikeTM, and OsecoTM.
  • the relief device also comprises a downstream relief valve 330 separated by a short pipe spool 331 from the rupture disk holder. The placement of the rupture disk upstream of the relief valve serves to prevent fouling of the relief valve inlet port and also minimizes potential emissions should the relief valve fail to maintain a seal under normal operating conditions.
  • the relief device assembly also includes a pressure gauge 333 connected to a pipe spool 331; this gauge provides an external indication of a pressure change between the rupture disk and the valve, thereby signaling when the rupture disk has burst and when changeout is required.
  • the flush ring 335 is installed upstream (below) and adjacent to the second annular member 307 of the rupture disk holder and may be held in place with through-bolting or other conventional means (not shown).
  • a supply of flushing fluid is connected to the ring via a conduit 337 and the flushing fluid flows into an internal channel of the ring.
  • the internal channel is annular and distributes the flushing fluid to a plurality of ports, located radially along the inner circumference of the flush ring.
  • one set of ports is positioned at a first orientation angle with respect to the axis of the ring and another set of ports is positioned at a second (different) orientation angle with respect to the axis of the ring.
  • FIG 4 is a partly sectional view of a first embodiment of a flush ring 435 in accord with the present invention, such as was utilized in the assembly of Fig. 3.
  • the flush ring 435 comprises an annular member 439 including a plurality of fluid ports 411 in its interior face 413 through which a flushing fluid may be passed.
  • the ports 411 are oriented at two different angles with respect to axis 415 of the annular member 439 in order to direct the flushing fluid (illustrated by the arrows) toward multiple points along the surface of a rupture disk (not shown).
  • the flushing fluid is supplied via a connection 419 to a source of flushing fluid (not shown) and an annular internal channel 421 which is operably connected to each of the ports 411 by respective feed channels 423.
  • FIG. 5 is a partly sectional view of a second embodiment of a flush ring 535 in accord with the present invention, such as can be utilized in the assembly of Fig. 3.
  • the flush ring 535 comprises an annular member 539 and an annular disk 541.
  • the annular member 539 includes a plurality of fluid ports 511 in it interior face 513 through which a flushing fluid may be passed.
  • the ports 511 are oriented at two different angles with respect to the axis 515 of the annular member 539 in order to direct the flushing fluid (illustrated by the arrows) toward multiple points along the surface of a rupture disk (not shown).
  • the flushing fluid is supplied via a connection 519 to a source of flushing fluid (not shown) and an annular internal channel 521 which is operably connected to each of the ports 511 by respective feed channels 523.
  • the annular disk 541 preferably has an inner diameter ID equal to that of annular member 539.
  • the annular disk 541 preferably has an outer diameter OD equal to that of annular member 539.
  • the annular disk 541 is fluid tightly sealed (e.g., as by welding) to the lower face 543 of annular member 539 so as to fluid tightly close the annular internal channel 521 so as to assure that there is no leakage of flushing fluid therefrom.
  • FIG. 6 is a partly sectional view of a still further embodiment of a rupture disk assembly 601, in accord with the present invention, which comprises a rupture disk 603 contained in a two-piece rupture disk holder comprising a first annular member 605 disposed in a downstream position relative to the rupture disk 603 and a third annular member 607 disposed in an upstream position relative to the rupture disk 603.
  • An outer peripheral portion 609 of the rupture disk 603 is sandwiched between the first annular member 605 and the third annular member 607.
  • a flush ring 635 comprising a second annular member 639 and an annular disk 641, fluid tightly sealed thereto, is disposed in an upstream position relative to the third annular member 607.
  • the third annular member 607 is sandwiched between the outer peripheral portion 609 of the rupture disk 603 and the flush ring 635.
  • a gasket 645 is interposed between the third annular member 607 and the flush ring 635 so as to ensure a fluid tight seal therebetween.
  • the second annular member 639 includes a plurality of fluid ports 611 in its interior face 613 through which a flushing fluid may be passed.
  • the ports 611 are oriented at two different angles with respect to axis 615 of the second annular member 639 in order to direct the flushing fluid (illustrated by the arrows) toward multiple points along the lower surface 617 of the rupture disk 603.
  • the flushing fluid is supplied via a connection 619 to a source of flushing fluid (not shown) and a closed annular internal channel 621 which is operably connected to each of the ports 611 by respective feed channels 623.
  • the low flow region 727 is within a short section of piping 732 adjacent to a valve 747 in the exit line 749 for a hydrogen cyanide reactor 751.
  • the valve can be opened, allowing the hydrogen cyanide containing product gas to be diverted to a flare for safe destruction.
  • the valve 747 is closed, creating a low-flow region at its face that could accumulate unwanted material, such as cyanide polymer.
  • Suitable flushing fluids may include but are not limited to N 2 , SO 2 , steam, CH 4 , H 2 and air.
  • the flushing fluid may optionally be heated and the flow rate of the fluid may be varied, if desired.
  • the low flow region 827 is in the pressure relief line 853 on a chemical reactor 855, e.g., a batch emulsion polymerization reactor.
  • a rupture disk 803 is installed in the horizontal portion of the pressure relief line and, over the course of a batch polymerization, vapor phase monomers may accumulate in the relief line upstream of the rupture disk.
  • a flush ring 835 of the present invention adjacent to the rupture disk, as shown, an introducing a flushing fluid comprising cleaning solvent following the completion of each batch, the rupture disk and the relief line are regularly cleared and remain free of unwanted material accumulation.
  • the low flow region 927 is within the blinded bottom cleanout connection 957 on a liquid filled crude product tank 959.
  • the blind 961 is present on the cleanout connection to provide a liquid-tight seal on the tank.
  • Various unwanted materials such as precipitates, corrosion products, insoluble impurities, and the like may also be present.
  • Suitable flushing fluids may include N 2 , air or a slip stream of crude product.
  • the flushing fluid may be a gas or a liquid ana may be supplied continuously or intermittently, as required. Any gas or liquid material compatible with the operation of the particular process in question may be used as the flushing fluid.
  • suitable materials include, but are not limited to, oxygen-containing gas (e.g., air), vapor phase polymerization inhibitors, water, (meth)acrylic acid, methyl-isobutyl-ketone (MIBK), toluene and acetone.
  • the flushing fluid may comprise distillation column reflux or unpurified distillation column feed.
  • the flushing fluid may optionally be passed through a heat exchanger to control its temperature and may optionally comprise one or more polymerization inhibitors.
  • the flush ring may comprise one or more ports and that the ports may be at one or more orientation angles with respect to the axis of the flush ring. Suitable orientation angles are between 0 and 90 degrees with respect to the axis of the flush ring.
  • the selection of orientation angles, as well as the size and number of ports, and the flushing fluid flow rate are a function of the internal diameter of the flush ring, the orientation of the surface to be treated (e.g., in the case of a rupture disk whether the surface is concave or convex) and the distance between the ports and the surface to be treated.
  • both the flush ring and the relevant element of process equipment can be repeatably assembled in the same configuration in the laboratory as is required in the process, thus allowing one of ordinary skill in the art to verify, in the laboratory, that the proper design variables have been selected through simple visual observation under flush fluid flow conditions. For example, if water is used as the flush fluid, it would be apparent that the proper variables have been selected when, by visual observation under operating conditions, the rupture disk is determined to be completely wetted by the water flush.
  • a flush ring is placed adjacent to the rupture disk holder on the 20.3 cm (8-inch) diameter top process connection nozzle of an acrylic acid distillation column in the manner as shown in Fig. 3.
  • a 316-teflon-316 composite rupture disk (available from Continental Disc Corp.TM) was installed in the holder.
  • the flush ring had an internal diameter 19.1 cm (7-1/2 inches)and comprised two sets of fluid ports.
  • the first set of ports comprises 8 equally spaced 0.238 cm (3/32-inch) diameter ports set at an angle of between 45 and 90 degrees relative to the axis of the ring.
  • the second set of ports comprises 8 equally spaced 0.238 cm (3/32-inch) diameter ports set at an angle between 0 and 45 degrees relative to the axis of the ring.
  • the flushing ring further comprises an open distribution channel which is sealed upon installation against a standard gasket flange. After installation, a flushing fluid is introduced through the ring which facilitates the removal of condensed polymerizable acrylic acid monomer from the upstream (lower) interior surfaces of the rupture isk, thereby preventing accumulation of unwanted polymer.
  • the flushing fluid is a liquid mixture comprising acrylic acid (distillation column feed), acetic acid and hydroquinone inhibitor, and is supplied at a continuous flow rate of approximately 7.57 liters/min (2 gpm) Oxygen-containing gas is present in the column vapor spaces as a routine aspect of operating the distillation column.
  • the acrylic acid distillation column was operated with the flush ring in this configuration for 6 months during which time the disk and process connection nozzle were inspected a total of 5 times. During each inspection, both the disk and the process nozzle connection were inspected and found to be free of polymer accumulation.
  • a single 0,953 cm (3/8-inch Spiraljet)® full-cone spray nozzle was installed in the manner as shown in Fig. 10 in an attempt to prevent polymer accumulation on the aforementioned composite rupture disk.
  • a pressurized liquid mixture comprising acrylic acid (distillation column feed), acetic acid and hydroquinone inhibitor were supplied at a continuous flow rate of approximately 7.57 liters/min (2 gpm) to the Spiraljet ® spray nozzle and subsequently sprayed into the process connection nozzle and onto the lower portion of the rupture disk.
  • Oxygen-containing gas is present in the column vapor spaces as a routine aspect of operating the distillation column.
  • the acrylic acid distillation column was operated with this configuration during which time the disk and process connection nozzle were inspected several times. Over varying operating periods - some as short as three weeks - significant amounts of polymer were found to have accumulated within the process connection nozzle and on the rupture disk itself, requiring the process connection nozzle to be cleaned and the rupture to be replaced. Typically, the process connection nozzle cross-section was found to be 60 - 90% obstructed with polymer, when inspected.

Landscapes

  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Safety Valves (AREA)
  • Paper (AREA)
  • Valve Housings (AREA)
  • Laminated Bodies (AREA)
  • Filling Or Discharging Of Gas Storage Vessels (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Polymerisation Methods In General (AREA)
  • Holding Or Fastening Of Disk On Rotational Shaft (AREA)

Abstract

In one embodiment, the invention provides a rupture disk assembly (101) having a rupture disk (103) and a rupture disk holder. The rupture disk holder has a first annular member (105) downstream of the rupture disk (103), a second annular member (107) upstream of the rupture disk (103), and an optional third annular member upstream of the second annular member. An outer peripheral portion (109) of the rupture disk (103) is sandwiched between the first and second annular members (105,107); and, if a third annular member is present, (a) the second annular member is sandwiched between the outer peripheral portion of the rupture disk and the third annular member, and (b) the third annular member includes a fluid port aimed at the rupture disk. However, if the third annular member is not present, the second annular member (107) includes a fluid port (123) aimed at the rupture disk (103). In another embodiment, the invention provides an equipment access assembly having an equipment access cover, an equipment access cover mount, and an annular member between the equipment access cover and cover mount. The annular member includes a fluid port aimed at the equipment access cover. In yet another embodiment, the invention provides a valve mounting assembly having a downstream valve mount, an upstream valve mount, a valve intermediate the downstream and upstream valve mounts, and an annular member intermediate the valve and the upstream valve mount. The annular member includes a fluid port aimed at the valve. <IMAGE>

Description

  • The accumulation of unwanted material in low flow regions of process equipment is a problem which adversely affects the chemical process industries on a daily basis. Unwanted materials may comprise byproducts, residues, polymers, scale, dusts, corrosion products, precipitates, or other solids, liquids or vapors. Unwanted materials may restrict process flows, initiate undesirable side reactions (such as stress corrosion cracking), seed polymer growth, and render secondary process devices - such as valves and instrumentation - inoperable. The accumulation of unwanted material is costly in that it requires process downtime and manpower to remove these materials and to repair associated damage to the process equipment and piping that may have occurred. In addition, hazardous situations can result when safety equipment, such as pressure relief devices, are isolated from the process through the accumulation of unwanted materials in the process connections to which they are attached.
  • A pressure relief device is disclosed in DE 31 02 828. The device comprises a rupture disk retained between two annular rings. The rupture disk extends across and seals a fluid conduit.
  • In the chemical process industries, one especially prevalent category of unwanted material accumulation is the formation of "condensation polymer". Condensation polymer forms when vapor-phase monomers condense onto equipment surfaces in the absence of suitable polymerization inhibitors and then undergo polymerization. Monomers known to undergo condensation polymerization include but are not limited to (meth)acrylic acid and its esters, vinyl chloride, hydrogen cyanide, acrylonitrile, styrene, and other vinyl monomers.
  • One known method for combating condensation polymerization in the vapor spaces of process equipment such as storage tanks, reaction kettles and distillation columns, is to maintain the surface temperature of the equipment above the dew point of the monomer(s); jacketing, insulation and electric or steam tracing of process equipment has been shown to be relatively effective in "open-flow" regions, i.e. regions where the vapor-phase monomer can freely flow away from the heated surfaces. This approach is ineffective, however, in low flow regions such as process connections where the monomer vapors can stagnate and become trapped; this situation is further exacerbated when the process connection is a vessel nozzle, oriented vertically on the top head of the process equipment in question.
  • Addition of vapor-phase inhibitors has also been tried as a means for preventing condensation polymerization inside process equipment such as distillation columns. Examples of such inhibitors include SO2 in hydrogen cyanide service and NPH in (meth)acrylic acid service. Because low flow regions, such as nozzles, are essentially stagnant, however, vapor-phase inhibitors tend not to flow into them and unwanted material accumulation can proceed essentially unabated.
  • Another method for combating condensation polymerization in the vapor spaces of process equipment is through the use of internal spray devices. European Published Patent Application No. 1 044 957 A1 teaches the use of a "spraying and supplying means" placed inside a distillation column to spray liquid on interior surfaces of the distillation column, with the intent of inhibiting polymer formation. By design, however, this type of spray device is most effective in addressing polymer growth in large, open-flow regions, such as the top head o a distillation column or storage tank. This approach fails to adequately prevent the simultaneous accumulation of material in small, low-flow regions, such as the process connections on the top heads of tanks and columns.
  • In those cases where accumulations must also be prevented in small process connections, such as vessel nozzles, European Published Patent Application No. 1 044 957 A1 suggests that one or more spray nozzles may additionally be employed to specifically spray these connections. Figure 10 of the present application illustrates such an embodiment wherein a spraying and supplying means is employed in combination with a top head connection to which a relief device (typically a rupture disk and relief valve assembly) is attached. The insertion of a single spray nozzle into the process connection from below is illustrated; in this configuration, a liquid spray would be direct upward into the stagnant process connection. The installation of the spray nozzle is mechanically complex as well as invasive to the vessel, requiring a separate vessel penetration (not shown) and the positioning of the line(s) inside the vessel for supplying the liquid to the spray nozzle. With this approach, the elevation and alignment of the spray nozzle itself, as well as the flow rate and spray pattern, are critical and, in practice, it is quite difficult to obtain the proper combination of these variables such that polymer accumulation is wholly prevented. While the effectiveness of such an arrangement could be improved through the use of multiple spray nozzle and an overwhelmingly large quantity of liquid spray, such an approach is costly and impractical in commercial operations. Additionally, the physical presence of the spray nozzle(s) and its supply line(s) create an undesirable obstruction in the process connection, thereby interfering with the free flow of material through the attached relief device, and these components themselves also create new surfaces for the accumulation of condensation polymer! In some instances the direct impingement of pressurized spray liquid on the relief device may also cause mechanical fatigue, thereby shortening the service life of the rupture disk. Because of these limitations, the proposed process for inhibiting polymerization is impractical when applied to the small, low flow regions associated with process connections, such as relief lines.
  • The use of spray rings of various designs is also known in the art as a means for cleaning the inside surfaces of sight glasses. Numerous patents have been issued for these devices and enhancements thereto, including U.S. Patent No. 3,402,418, U.S. Patent No. 4, 158,508 and U.S. Patent No. 4,541,277. Yet despite familiarity with the needs of the chemical process industries, those skilled in the art of designing sight glass spray rings have not anticipated the use of such devices for the prevention o unwanted material accumulation in low flow zones such as process connections.
  • In fact, despite these known methods, there remains a long-felt need to provide a simplified, reliable, inexpensive and effective means for preventing unwanted material accumulation in low flow regions, such as process connections. This need is especially great in the case where safety relief systems are attached to process connections comprising low flow regions; the accumulation of unwanted material in these nozzles restricting the free flow of material through the nozzle when the relief device is called upon to operate, thereby limiting the capacity of the relief device and creating an unsafe condition. The present invention overcomes the deficiencies of the prior art while meeting the needs of the chemical process industries.
  • According to the present invention, there is provided a rupture disk assembly comprising a rupture disk and a rupture disk holder operatively engaging the rupture disk; wherein the rupture disk holder comprises a first annular member disposed in a downstream position relative to the rupture disk and a second annular member disposed in an upstream position relative to the rupture disk; wherein an outer peripheral portion of the rupture disk is sandwiched between the first annular member and the second annular member; wherein the second annular member includes at least one fluid port aimed at the rupture disk.
  • Alternatively, in a second embodiment of the present invention, there is provided a rupture disk assembly comprising a rupture disk and a rupture disk holder operatively engaging the rupture disk; wherein the rupture disk holder comprises a first annular member disposed in a downstream position relative to the rupture disk, a second annular member disposed in an upstream position relative to said rupture disk and a third annular member disposed in an upstream position relative to the rupture disk; wherein an outer peripheral portion of the rupture disk is sandwiched between the first annular member and the third annular member; wherein the third annular member is sandwiched between the outer peripheral portion of the rupture disk and the second annular member; wherein the second annular member includes at least one fluid port aimed at the rupture disk.
  • Figure 1 is a partly sectional view of a rupture disk assembly in accord with the present invention.
  • Figure 2 is a partly sectional view of another embodiment of a rupture disk assembly in accord with the present invention.
  • Figure 3 is a partly sectional view of a relief device assembly in accord with the present invention.
  • Figure 4 is a partly sectional view of a first embodiment of a flush ring in accord with the present invention.
  • Figure 5 is a partly sectional view of a second embodiment of a flush ring in accord with the present invention.
  • Figure 6 is a partly sectional view of a still further embodiment of a rupture disk assembly in accord with the present invention.
  • Figure 7 is a partly sectional view of a valve mounting assembly which does not form part of the present invention.
  • Figure 8 is a partly sectional view of a rupture disk assembly of the type shown in Fig. 1 disposed in the pressure relief line on a chemical reactor in accord with the present invention.
  • Figure 9 is a partly sectional view of a flush ring mounted in the bottom cleanout connection of a liquid filled crude-product tank which does not form part of the present invention.
  • Figure 10 is a partly sectional view of a relief device assembly using a spray nozzle system.
  • In the drawing figures, similar elements are similarly numbered.
  • In the following description, by "process equipment" is meant vessels, such as distillation columns, tanks and reactors, and process piping systems. By "process connections" is meant any extension of process equipment which can be utilized for the attachment of secondary process devices such as valves, instrumentation, pumps or pressure relief devices. Process connections include, but are not limited to, studding outlets, piping branches (e.g., piping tees), manways, handholes and flanged nozzles.
  • As will become apparent hereinafter, a key component of the present invention is a flush ring, i.e. an annular member having one or more fluid ports, the one or more fluid ports serving to direct a flushing fluid inwardly of said annular device, preferably toward the axis of the annulus. The annular member also includes an internal channel fluidically connecting the one or more ports to an external source of the flushing fluid. It is preferred that the annular member be of a constant external diameter. It is also preferred that the annular member be of a constant internal diameter. It is further preferred that the annular member comprises smooth and substantially parallel upper and lower surfaces of such a quality as to facilitate sealing when installed with conventional gaskets in a piece of process equipment.
  • Any gaseous or liquid material, compatible with the operation of the process, may be employed as the flushing fluid. The flushing fluid may be supplied continuously or intermittently, as required.
  • When installed in a low flow region, the flush ring serves to flush unwanted materials from the low flow region, thereby preventing their accumulation and avoiding the previously described processing difficulties associated with the accumulation of unwanted materials.
  • The flush ring may be optionally installed with a flow measurement / control device (such as a control valve, a needle valve or a rotometer) on the flush fluid supply connection. This serves to ensure proper flushing fluid flow is maintained at all times, as intended.
  • Figure 1 illustrates one embodiment of a flush ring in accord with the present invention. In this embodiment, an annular channel and fluid ports consistent with the present invention are incorporated directly into a rupture disk holder. In so doing, a fluid flush may be provided to prevent the accumulation of unwanted material, such as condensation polymer, in the low flow region upstream of a rupture disk.
  • The rupture disk assembly 101 is representative of conventional assemblies used in industrial chemical processes and comprises a rupture disk 103 contained in a two-piece rupture disk holder comprising a first annular member 105 disposed in a downstream position relative to the rupture disk 103 and a second annular member 107 disposed in an upstream position relative to the rupture disk 103. An outer peripheral portion 109 of the rupture disk 103 is sandwiched between the first annular member 105 and the second annular member 107. In accordance with the present invention, however, the second annular member 107 includes a plurality of fluid ports 111 in its interior face 113 through which a flushing fluid may be passed. The ports 111 are oriented at two different angles with respect to the axis 115 of the second annular member 107 in order to direct the flushing fluid (illustrated by the arrows) toward multiple points along the lower surface 117 of the rupture disk 103. The flushing fluid is supplied via a connection 119 to a source of flushing fluid (not shown) and an annular internal channel 121 which is operably connected to each of the ports 111 by respective feed channels 123.
  • Figure 2 illustrates an embodiment of the flush ring in accord with the present invention wherein only two fluid ports are utilized. In particular, fluid port 211a is oriented at a first angle with respect to the axis 215 of the second annular member 207 and conducts flushing fluid (illustrated by the arrow) toward a first area on the lower surface 217 of the rupture disk 203. Fluid port 211a is supplied via a radially-oriented hole 225a and feed channel 223a in the second annular member 207. The radially-oriented hole 225a serves to conduct flushing fluid from the connector 219a which is in turn connected to a source of flushing fluid (not shown). Similarly, fluid port 211b (located on the diametrically opposite side of the second annular member) is oriented at a second angle (different from the first angle) with respect to the axis 215 and flushing fluid toward a second area on the lower surface 217 of the rupture disk 203. Fluid port 211b is supplied via a radially-oriented hole 225b and feed channel 223b in the second annular member 207. The radially-oriented hole 225b serves to conduct flushing fluid from the connector 219b which is in turn connected to a source of flushing fluid (not shown).
  • Connector 219a and connector 219b may draw flushing fluid from the same source or may optionally use different flushing fluids - for example, one fluid may comprise water and the other fluid may comprise an organic solvent such as hexane, or alternatively, one fluid may comprise phenolic inhibitor solution and the other may comprise an oxygen-containing gas.
  • Figure 3 illustrates another embodiment of the flush ring in accord with the present invention which, while functionally similar to the apparatus of Figs. 1 and 2, is an independent part. This independent flush ring is used to prevent the accumulation of unwanted material, such as condensation polymer, in the low flow region, generally indicated as 327, upstream of a relief device assembly, generally indicated as 329. The relief device assembly 329 is representative of conventional assemblies used in industrial chemical processes, one example of which is described in U.S. Patent No. 6,311,715. The relief device assembly in this preferred embodiment comprises a reverse-buckling rupture disk 304 (contained in a two-piece rupture disk holder comprising a first annular member 305 and a second annular member 307). Suitable reverse-buckling rupture disks are commercially available from Continental Disc Corporation™, Fike™, and Oseco™. The relief device also comprises a downstream relief valve 330 separated by a short pipe spool 331 from the rupture disk holder. The placement of the rupture disk upstream of the relief valve serves to prevent fouling of the relief valve inlet port and also minimizes potential emissions should the relief valve fail to maintain a seal under normal operating conditions.
  • The relief device assembly also includes a pressure gauge 333 connected to a pipe spool 331; this gauge provides an external indication of a pressure change between the rupture disk and the valve, thereby signaling when the rupture disk has burst and when changeout is required. In this embodiment, the flush ring 335 is installed upstream (below) and adjacent to the second annular member 307 of the rupture disk holder and may be held in place with through-bolting or other conventional means (not shown). A supply of flushing fluid is connected to the ring via a conduit 337 and the flushing fluid flows into an internal channel of the ring. The internal channel is annular and distributes the flushing fluid to a plurality of ports, located radially along the inner circumference of the flush ring. In this embodiment, one set of ports is positioned at a first orientation angle with respect to the axis of the ring and another set of ports is positioned at a second (different) orientation angle with respect to the axis of the ring. As flushing fluid is ejected through the ports, it is directed upward, toward the exposed upstream surfaces of the rupture disk, as shown by the arrows, thereby displacing the otherwise stagnant contents of low flow region 327 and preventing the accumulation of unwanted materials in this region.
  • Figure 4 is a partly sectional view of a first embodiment of a flush ring 435 in accord with the present invention, such as was utilized in the assembly of Fig. 3. In particular, the flush ring 435 comprises an annular member 439 including a plurality of fluid ports 411 in its interior face 413 through which a flushing fluid may be passed. The ports 411 are oriented at two different angles with respect to axis 415 of the annular member 439 in order to direct the flushing fluid (illustrated by the arrows) toward multiple points along the surface of a rupture disk (not shown). The flushing fluid is supplied via a connection 419 to a source of flushing fluid (not shown) and an annular internal channel 421 which is operably connected to each of the ports 411 by respective feed channels 423.
  • Figure 5 is a partly sectional view of a second embodiment of a flush ring 535 in accord with the present invention, such as can be utilized in the assembly of Fig. 3. In particular, the flush ring 535 comprises an annular member 539 and an annular disk 541. The annular member 539 includes a plurality of fluid ports 511 in it interior face 513 through which a flushing fluid may be passed. The ports 511 are oriented at two different angles with respect to the axis 515 of the annular member 539 in order to direct the flushing fluid (illustrated by the arrows) toward multiple points along the surface of a rupture disk (not shown). The flushing fluid is supplied via a connection 519 to a source of flushing fluid (not shown) and an annular internal channel 521 which is operably connected to each of the ports 511 by respective feed channels 523. The annular disk 541 preferably has an inner diameter ID equal to that of annular member 539. Similarly, the annular disk 541 preferably has an outer diameter OD equal to that of annular member 539. The annular disk 541 is fluid tightly sealed (e.g., as by welding) to the lower face 543 of annular member 539 so as to fluid tightly close the annular internal channel 521 so as to assure that there is no leakage of flushing fluid therefrom.
  • Figure 6 is a partly sectional view of a still further embodiment of a rupture disk assembly 601, in accord with the present invention, which comprises a rupture disk 603 contained in a two-piece rupture disk holder comprising a first annular member 605 disposed in a downstream position relative to the rupture disk 603 and a third annular member 607 disposed in an upstream position relative to the rupture disk 603. An outer peripheral portion 609 of the rupture disk 603 is sandwiched between the first annular member 605 and the third annular member 607. A flush ring 635, comprising a second annular member 639 and an annular disk 641, fluid tightly sealed thereto, is disposed in an upstream position relative to the third annular member 607. The third annular member 607 is sandwiched between the outer peripheral portion 609 of the rupture disk 603 and the flush ring 635. A gasket 645 is interposed between the third annular member 607 and the flush ring 635 so as to ensure a fluid tight seal therebetween. The second annular member 639 includes a plurality of fluid ports 611 in its interior face 613 through which a flushing fluid may be passed. The ports 611 are oriented at two different angles with respect to axis 615 of the second annular member 639 in order to direct the flushing fluid (illustrated by the arrows) toward multiple points along the lower surface 617 of the rupture disk 603. The flushing fluid is supplied via a connection 619 to a source of flushing fluid (not shown) and a closed annular internal channel 621 which is operably connected to each of the ports 611 by respective feed channels 623.
  • Although the majority of the preceding discussion is focused on flanged nozzles attached to process vessels, it is envisioned that other low flow regions may also benefit from the present invention.
  • In one embodiment which does not form part of the present invention (see Figure 7), the low flow region 727 is within a short section of piping 732 adjacent to a valve 747 in the exit line 749 for a hydrogen cyanide reactor 751. During process upsets, the valve can be opened, allowing the hydrogen cyanide containing product gas to be diverted to a flare for safe destruction. Under normal operating conditions, the valve 747 is closed, creating a low-flow region at its face that could accumulate unwanted material, such as cyanide polymer. By placing a flush ring 735 adjacent to the valve, as shown, and introducing a flushing fluid via the ring, the accumulation of unwanted materials is prevented and operability of the valve is maintained. Suitable flushing fluids may include but are not limited to N2, SO2, steam, CH4, H2 and air. The flushing fluid may optionally be heated and the flow rate of the fluid may be varied, if desired.
  • In another embodiment (see Figure 8), the low flow region 827 is in the pressure relief line 853 on a chemical reactor 855, e.g., a batch emulsion polymerization reactor. A rupture disk 803 is installed in the horizontal portion of the pressure relief line and, over the course of a batch polymerization, vapor phase monomers may accumulate in the relief line upstream of the rupture disk. By placing a flush ring 835 of the present invention adjacent to the rupture disk, as shown, an introducing a flushing fluid comprising cleaning solvent following the completion of each batch, the rupture disk and the relief line are regularly cleared and remain free of unwanted material accumulation.
  • In another embodiment which does not form part of the present invention (see Figure 9), the low flow region 927 is within the blinded bottom cleanout connection 957 on a liquid filled crude product tank 959. Under normal conditions, the blind 961 is present on the cleanout connection to provide a liquid-tight seal on the tank. Various unwanted materials such as precipitates, corrosion products, insoluble impurities, and the like may also be present. During maintenance periods, it is desirable to remove the blind and to use the drain connection as a conduit through which the contents of the tank may be removed. By placing a flush ring 935 adjacent to the blind, as shown, and introducing a flushing fluid via the ring, the accumulation of unwanted material is prevented and the drain connection is ready for use on demand. Suitable flushing fluids may include N2, air or a slip stream of crude product.
  • It is understood that the flushing fluid may be a gas or a liquid ana may be supplied continuously or intermittently, as required. Any gas or liquid material compatible with the operation of the particular process in question may be used as the flushing fluid. For example, in the operation of a distillation column for the production of (meth)acrylic acid or esters thereof, suitable materials include, but are not limited to, oxygen-containing gas (e.g., air), vapor phase polymerization inhibitors, water, (meth)acrylic acid, methyl-isobutyl-ketone (MIBK), toluene and acetone. In some embodiments, the flushing fluid may comprise distillation column reflux or unpurified distillation column feed. The flushing fluid may optionally be passed through a heat exchanger to control its temperature and may optionally comprise one or more polymerization inhibitors.
  • It is further understood that the flush ring may comprise one or more ports and that the ports may be at one or more orientation angles with respect to the axis of the flush ring. Suitable orientation angles are between 0 and 90 degrees with respect to the axis of the flush ring. The selection of orientation angles, as well as the size and number of ports, and the flushing fluid flow rate are a function of the internal diameter of the flush ring, the orientation of the surface to be treated (e.g., in the case of a rupture disk whether the surface is concave or convex) and the distance between the ports and the surface to be treated. Because of their designs, both the flush ring and the relevant element of process equipment (e.g., the rupture disk holder) can be repeatably assembled in the same configuration in the laboratory as is required in the process, thus allowing one of ordinary skill in the art to verify, in the laboratory, that the proper design variables have been selected through simple visual observation under flush fluid flow conditions. For example, if water is used as the flush fluid, it would be apparent that the proper variables have been selected when, by visual observation under operating conditions, the rupture disk is determined to be completely wetted by the water flush.
  • With the benefit of the disclosure of the present invention, it is envisioned that for certain process uses the benefits of the flush ring can be reasonably well approximated through the installation of a commercially available spray ring device. Such spray ring devices are marketed for the purpose of cleaning sight glasses and may be purchased in standard sizes from LJStar Inc™. (Twinsburg, OH) or Canty™ (Buffalo, NY). Because these devices are designed for a different purpose, use of the aforementioned visual test method I essential to verify that the selected "standard" device can meet the requirements of the process service.
  • Example
  • A flush ring is placed adjacent to the rupture disk holder on the 20.3 cm (8-inch) diameter top process connection nozzle of an acrylic acid distillation column in the manner as shown in Fig. 3. A 316-teflon-316 composite rupture disk (available from Continental Disc Corp.™) was installed in the holder. The flush ring had an internal diameter 19.1 cm (7-1/2 inches)and comprised two sets of fluid ports. The first set of ports comprises 8 equally spaced 0.238 cm (3/32-inch) diameter ports set at an angle of between 45 and 90 degrees relative to the axis of the ring. The second set of ports comprises 8 equally spaced 0.238 cm (3/32-inch) diameter ports set at an angle between 0 and 45 degrees relative to the axis of the ring. The flushing ring further comprises an open distribution channel which is sealed upon installation against a standard gasket flange. After installation, a flushing fluid is introduced through the ring which facilitates the removal of condensed polymerizable acrylic acid monomer from the upstream (lower) interior surfaces of the rupture isk, thereby preventing accumulation of unwanted polymer. The flushing fluid is a liquid mixture comprising acrylic acid (distillation column feed), acetic acid and hydroquinone inhibitor, and is supplied at a continuous flow rate of approximately 7.57 liters/min (2 gpm) Oxygen-containing gas is present in the column vapor spaces as a routine aspect of operating the distillation column. The acrylic acid distillation column was operated with the flush ring in this configuration for 6 months during which time the disk and process connection nozzle were inspected a total of 5 times. During each inspection, both the disk and the process nozzle connection were inspected and found to be free of polymer accumulation.
  • Comparative Example
  • On the same 20.3 cm (8-inch) diameter top process connection nozzle, a single 0,953 cm (3/8-inch Spiraljet)® full-cone spray nozzle (Spraying Systems Co™., Wheaton, Ill.) was installed in the manner as shown in Fig. 10 in an attempt to prevent polymer accumulation on the aforementioned composite rupture disk. A pressurized liquid mixture comprising acrylic acid (distillation column feed), acetic acid and hydroquinone inhibitor were supplied at a continuous flow rate of approximately 7.57 liters/min (2 gpm) to the Spiraljet ® spray nozzle and subsequently sprayed into the process connection nozzle and onto the lower portion of the rupture disk. Oxygen-containing gas is present in the column vapor spaces as a routine aspect of operating the distillation column. The acrylic acid distillation column was operated with this configuration during which time the disk and process connection nozzle were inspected several times. Over varying operating periods - some as short as three weeks - significant amounts of polymer were found to have accumulated within the process connection nozzle and on the rupture disk itself, requiring the process connection nozzle to be cleaned and the rupture to be replaced. Typically, the process connection nozzle cross-section was found to be 60 - 90% obstructed with polymer, when inspected.

Claims (6)

  1. A rupture disk assembly comprising:
    (i) a rupture disk (103); and
    (ii) a rupture disk holder operatively engaging said rupture disk (103);
       wherein said rupture disk holder comprises:
    (a) a first annular member (105) disposed in a downstream position relative to said rupture disk (103); and
    (b) a second annular member (107) disposed in an upstream position relative to said rupture disk (103);
       wherein an outer peripheral portion of said rupture disk (103) is
       sandwiched between said first annular member (105) and said second annular member (107);
       characterized in that said second annular member (107) includes at least one fluid port (111) aimed at said rupture disk (103).
  2. The rupture disk assembly according to claim 1, wherein said second annular member (107) includes a plurality of fluid ports (111) aimed at said rupture disk (103).
  3. The rupture disk assembly according to claim 1, wherein said first annular member (105) has an axis (115), said second annular member (107) has an axis (115), and said first annular member (105) and said second annular member (107) are coaxially disposed with respect to one another.
  4. The rupture disk assembly according to claim 1, wherein an inside diameter of said first annular member (105) is constant, an inside diameter of said second annular member (107) is constant, and said inside diameter of said first annular member (105) is equal to said inside diameter of said second annular member (107).
  5. The rupture disk assembly according to claim 1, wherein an outside diameter of said first annular member (105) is constant, an outside diameter of said second annular member (107) is constant, and said outside diameter of said first annular member (105) is equal to said outside diameter of said second annular member (107).
  6. The rupture disk assembly according to any preceding claim, further comprising:
    (c) a third annular member (607) disposed in an upstream position relative to said rupture disk (603);
       wherein an outer peripheral portion of said rupture disk (603) is sandwiched between said first annular member (605) and said third annular member (607);
    wherein said third annular member (607) is sandwiched between said outer peripheral portion of said rupture disk (603) and said second annular member (639).
EP20030253952 2002-07-05 2003-06-23 Rupture disc assembly Expired - Lifetime EP1378694B1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
EP05076038A EP1561521A3 (en) 2002-07-05 2003-06-23 Apparatus to prevent the accumulation of unwanted material
EP05077882A EP1640647A3 (en) 2002-07-05 2003-06-23 Valve mounting assembly

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US39401102P 2002-07-05 2002-07-05
US394011P 2002-07-05

Related Child Applications (1)

Application Number Title Priority Date Filing Date
EP05076038A Division EP1561521A3 (en) 2002-07-05 2003-06-23 Apparatus to prevent the accumulation of unwanted material

Publications (3)

Publication Number Publication Date
EP1378694A2 EP1378694A2 (en) 2004-01-07
EP1378694A3 EP1378694A3 (en) 2004-01-28
EP1378694B1 true EP1378694B1 (en) 2005-11-02

Family

ID=29720453

Family Applications (1)

Application Number Title Priority Date Filing Date
EP20030253952 Expired - Lifetime EP1378694B1 (en) 2002-07-05 2003-06-23 Rupture disc assembly

Country Status (13)

Country Link
US (3) US6983758B2 (en)
EP (1) EP1378694B1 (en)
JP (1) JP2004131179A (en)
KR (1) KR20040004180A (en)
CN (1) CN100439777C (en)
AT (1) ATE308703T1 (en)
AU (3) AU2003204925B2 (en)
BR (1) BR0302336B1 (en)
DE (1) DE60302109T2 (en)
MX (1) MXPA03006050A (en)
SG (1) SG113470A1 (en)
TW (1) TWI225135B (en)
ZA (1) ZA200305028B (en)

Families Citing this family (40)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8157969B2 (en) * 2006-06-01 2012-04-17 Rohm And Haas Company Method and apparatus for minimizing accumulation of polymer on process equipment, especially safety devices
RU2443716C2 (en) * 2006-06-01 2012-02-27 Джон О. БАРНЕТТ Method and apparatus for minimising polymer deposits on process equipment, particularly on protective devices
KR100677917B1 (en) * 2006-06-09 2007-02-06 윤하원 Rupture disc assembly
EP2049821A4 (en) 2006-07-21 2013-09-04 Amgen Inc Rupture valve
GB2441146A (en) * 2006-08-24 2008-02-27 Eco Rupture Disc Ltd Bursting disc mounting assembly with incorrect installation warning
FR2910584A1 (en) 2006-12-21 2008-06-27 Areva T & D Sa Pressure releasing device for electrical apparatus, has hinge part to connect cover and envelope, where cover pivots around axle of hinge part when cover is opened such that cover forms deflector for gas
KR100805263B1 (en) * 2006-12-26 2008-02-20 윤하원 Device for testing a rupture disk and method thereof
US8011381B2 (en) * 2008-10-02 2011-09-06 Applied Material, Inc. Balanced purge slit valve
US20100170573A1 (en) * 2009-01-06 2010-07-08 Draper Don R Pressure relief mechanism having a rupture disk
RU2489628C2 (en) * 2009-05-27 2013-08-10 Олег Савельевич Кочетов Kochetov explosion-proof device
DE102010014580A1 (en) * 2010-04-09 2011-10-13 Dieter Wurz Multi-fuel nozzle with primary gas jet
RU2459050C1 (en) * 2011-04-13 2012-08-20 Олег Савельевич Кочетов Method to select opening size for blast relief element of structure and its weight designed to protect buildings and structures against explosions
US10661316B2 (en) * 2011-05-27 2020-05-26 Schlumberger Technology Corporation Oilfield material metering gate obstruction removal system
BR112014005403A2 (en) * 2011-09-08 2017-03-28 Bs&B Safety Systems Ltd safety heads, safety head assemblies and their insertion member
US10214345B1 (en) * 2011-12-12 2019-02-26 Cameron Gordon Howie Entryway protective collar
US9199789B2 (en) * 2012-02-29 2015-12-01 Fike Corporation Explosion vent including buckle tab plate
WO2014105898A1 (en) 2012-12-26 2014-07-03 Applied Cavitation, Inc. Piezoelectric devices
US9133960B2 (en) * 2013-01-29 2015-09-15 Mks Instruments, Inc. Fluid control valves
RU2520670C1 (en) * 2013-04-02 2014-06-27 Олег Савельевич Кочетов Device of opening size selection for relief constructional element and its weight, designed to protect buildings and structures against explosions
CN104847962B (en) * 2014-02-14 2019-11-22 欧洲技术设于伊特根的三聚氰氨-卢森堡-分支机构 Switch valve, for producing the reactor of melamine, relevant device and purging method equipped with the valve
RU2651913C2 (en) * 2014-04-08 2018-04-24 Олег Савельевич Кочетов Kochetov blast valve
RU2552425C1 (en) * 2014-05-15 2015-06-10 Олег Савельевич Кочетов Device for selection of hole size for easy detachable element of construction and its mass, designed to protect buildings and structures from explosions
CN104019260B (en) * 2014-06-13 2016-08-17 北京北机机电工业有限责任公司 Electric detonation diaphragm valve
RU2582133C1 (en) * 2015-03-20 2016-04-20 Олег Савельевич Кочетов Vehicle-process explosion-proof container
RU2582134C1 (en) * 2015-03-20 2016-04-20 Олег Савельевич Кочетов Explosion-proof chamber
US20160341320A1 (en) * 2015-05-21 2016-11-24 Mark Taylor Cleaning mechanisms for check valves
RU2658951C2 (en) * 2015-10-16 2018-06-26 Мария Михайловна Стареева Safety collapsing construction of buildings fencing
RU2615228C1 (en) * 2016-05-20 2017-04-04 Олег Савельевич Кочетов Explosion-proof device with bursting disk by kochetov
RU2616090C1 (en) * 2016-05-27 2017-04-12 Олег Савельевич Кочетов Kochetov's method of explosive protection with emergency situation alert system
JP2018104591A (en) * 2016-12-27 2018-07-05 Jnc株式会社 Manufacturing method of vinyl chloride resin for preventing scale adhesion
RU2648093C1 (en) * 2017-02-27 2018-03-22 Олег Савельевич Кочетов Explosion-proof device for technological equipment
RU2648092C1 (en) * 2017-02-27 2018-03-22 Олег Савельевич Кочетов Method of explosion protection with system to alert personnel to initial phase of emergency situation
RU2646075C1 (en) * 2017-03-13 2018-03-01 Олег Савельевич Кочетов Method of explosion protection with system to alert personnel to initial phase of emergency situation
RU2648109C1 (en) * 2017-04-13 2018-03-22 Олег Савельевич Кочетов Method of determining the effectiveness of explosive protection with the alert system of the emergency situation
CN106931210B (en) * 2017-04-26 2023-02-28 珠海格力电器股份有限公司 Fusible plug and pressure equipment
RU2646121C1 (en) * 2017-05-23 2018-03-01 Олег Савельевич Кочетов Explosive protection element with the emergency alarm system
WO2020097541A1 (en) * 2018-11-09 2020-05-14 Flowserve Management Company Methods and valves including flushing features.
CN112108099A (en) * 2020-10-23 2020-12-22 山东诺为制药流体系统有限公司 Three-piece type baffle box and reactor
CN114682182A (en) * 2020-12-28 2022-07-01 中昊晨光化工研究院有限公司 Device system and method for producing polymer by gas phase method
CN113833985B (en) * 2021-09-15 2022-12-27 湖北弘仪电子科技股份有限公司 Explosion-proof assembly for pressure container

Family Cites Families (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3402418A (en) 1966-04-25 1968-09-24 Roy Gene Le Wiper assembly for sight glass
US3485082A (en) * 1968-11-26 1969-12-23 Black Sivalls & Bryson Inc Method for testing relief valves
US3768299A (en) * 1972-06-26 1973-10-30 Lee Tex Valve Inc Automatic test valve for testing pressure relief valves
BE830895A (en) * 1975-07-01 1976-01-02 DEVICE FOR MONITORING THE INTERIOR OF A SPEAKER
US4158508A (en) 1977-05-16 1979-06-19 Jacoby-Tarbox Corporation Sight glass and product cleaning system
FR2436927A1 (en) 1978-09-21 1980-04-18 Vinyle Sa Ste Artesienne DRAIN VALVE AND METHOD OF USING A DRAIN VALVE
US4263929A (en) * 1979-01-08 1981-04-28 Kearney John G Electropneumatic pressure relief indicator
DE3102828C2 (en) 1981-01-29 1983-03-24 Phönix Armaturen-Werke Bregel GmbH, 6000 Frankfurt Rupture foil safety valve
US4462420A (en) * 1982-06-14 1984-07-31 Teledyne Farris Engineering Safety pressure relief valve
US4557625A (en) * 1983-06-29 1985-12-10 Jahnke Richard P Internal sealing assembly
US4541277A (en) 1983-09-23 1985-09-17 Southwire Company Self-sealing, self-cleaning sight glass
CA2012964C (en) * 1990-01-09 1998-06-16 Edward H. Short Iii Scored reverse buckling rupture disk assembly
DE4210878A1 (en) 1992-04-01 1993-10-14 Abk Armaturenbau Gmbh Shut-off or diverter valve with piggable passage
GB9220407D0 (en) * 1992-09-28 1992-11-11 Courtaulds Plc Pipeline
US5579942A (en) * 1993-10-07 1996-12-03 Bs&B Safety Systems, Inc. Vacuum support and rupture disk assembly
US5934308A (en) * 1995-10-24 1999-08-10 Bs&B Safety Systems, Inc. Rupture disk apparatus and methods
JP3787261B2 (en) 1999-04-16 2006-06-21 株式会社日本触媒 Method for preventing polymerization of easily polymerizable compounds
US6311715B1 (en) 2000-07-07 2001-11-06 Zook Enterprises, Llc Stacked rupture disk assembly

Also Published As

Publication number Publication date
TWI225135B (en) 2004-12-11
AU2009200249A1 (en) 2009-02-12
MXPA03006050A (en) 2005-02-14
US7556055B2 (en) 2009-07-07
US20050252551A1 (en) 2005-11-17
AU2009200250A1 (en) 2009-02-12
CN1472462A (en) 2004-02-04
AU2003204925B2 (en) 2009-03-05
KR20040004180A (en) 2004-01-13
BR0302336A (en) 2004-08-17
EP1378694A2 (en) 2004-01-07
EP1378694A3 (en) 2004-01-28
DE60302109D1 (en) 2005-12-08
TW200406556A (en) 2004-05-01
AU2009200249B2 (en) 2010-03-25
US7128085B2 (en) 2006-10-31
US20040003842A1 (en) 2004-01-08
ZA200305028B (en) 2004-03-10
JP2004131179A (en) 2004-04-30
CN100439777C (en) 2008-12-03
SG113470A1 (en) 2005-08-29
US20070006535A1 (en) 2007-01-11
ATE308703T1 (en) 2005-11-15
BR0302336B1 (en) 2014-11-25
DE60302109T2 (en) 2006-08-03
AU2009200250B2 (en) 2010-03-25
US6983758B2 (en) 2006-01-10
AU2003204925A1 (en) 2004-01-22

Similar Documents

Publication Publication Date Title
EP1378694B1 (en) Rupture disc assembly
CA1294796C (en) Orifice plate assembly
KR100509449B1 (en) Method for handling easily polymerizable compound
TWI416027B (en) Self purging expansion joint
EP3171110B1 (en) Atmospheric distillation column overhead oil-gas heat exchange apparatus and heat exchange method
RU2468873C2 (en) Device and method for cyclone cleaning
RU2443716C2 (en) Method and apparatus for minimising polymer deposits on process equipment, particularly on protective devices
EP1561521A2 (en) Apparatus to prevent the accumulation of unwanted material
EP1640647A2 (en) Valve mounting assembly
US6989095B2 (en) Fluid conditioner for reducing scale, corrosion and paraffin buildup in hydrocarbon piping
US8157969B2 (en) Method and apparatus for minimizing accumulation of polymer on process equipment, especially safety devices
KR20160071334A (en) Quench-cooling system
US5512140A (en) In-service cleaning of columns
CA2666022C (en) Sour natural gas sparger
US20130153466A1 (en) Coker inlet design to minimize effects of impingement
US20170370615A1 (en) Apparatus and method for rapid drain of water heater

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

PUAL Search report despatched

Free format text: ORIGINAL CODE: 0009013

17P Request for examination filed

Effective date: 20030705

AK Designated contracting states

Kind code of ref document: A2

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IT LI LU MC NL PT RO SE SI SK TR

AX Request for extension of the european patent

Extension state: AL LT LV MK

AK Designated contracting states

Kind code of ref document: A3

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IT LI LU MC NL PT RO SE SI SK TR

AX Request for extension of the european patent

Extension state: AL LT LV MK

17Q First examination report despatched

Effective date: 20040323

AKX Designation fees paid

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IT LI LU MC NL PT RO SE SI SK TR

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IT LI LU MC NL PT RO SE SI SK TR

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CH

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20051102

Ref country code: IT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT;WARNING: LAPSES OF ITALIAN PATENTS WITH EFFECTIVE DATE BEFORE 2007 MAY HAVE OCCURRED AT ANY TIME BEFORE 2007. THE CORRECT EFFECTIVE DATE MAY BE DIFFERENT FROM THE ONE RECORDED.

Effective date: 20051102

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20051102

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20051102

Ref country code: CZ

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20051102

Ref country code: AT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20051102

Ref country code: BE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20051102

Ref country code: RO

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20051102

Ref country code: SI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20051102

Ref country code: SK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20051102

Ref country code: LI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20051102

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

REF Corresponds to:

Ref document number: 60302109

Country of ref document: DE

Date of ref document: 20051208

Kind code of ref document: P

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060202

Ref country code: BG

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060202

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060202

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060202

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060213

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060403

NLV1 Nl: lapsed or annulled due to failure to fulfill the requirements of art. 29p and 29m of the patents act
PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: HU

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20060503

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

ET Fr: translation filed
PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed

Effective date: 20060803

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: EE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20051102

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: TR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20051102

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20051102

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: IE

Payment date: 20090626

Year of fee payment: 7

Ref country code: MC

Payment date: 20090602

Year of fee payment: 7

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: LU

Payment date: 20090701

Year of fee payment: 7

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MC

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20100630

REG Reference to a national code

Ref country code: IE

Ref legal event code: MM4A

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20100623

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20100623

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 14

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 15

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 16

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20190612

Year of fee payment: 17

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20190619

Year of fee payment: 17

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20200512

Year of fee payment: 18

REG Reference to a national code

Ref country code: DE

Ref legal event code: R119

Ref document number: 60302109

Country of ref document: DE

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20200623

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20200623

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20210101

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20210630